Potassium N-bromo-2,4-dichloro­benzene­sulfonamidate sesquihydrate

Gowda, B.T.; Foro, S.; Spandana, H.S.

doi:10.1107/S1600536812042456

Volume 68
Part 11
Page m1368
November 2012

Received 2 October 2012
Accepted 10 October 2012
Online 20 October 2012

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.005 Å
R = 0.037
wR = 0.093
Data-to-parameter ratio = 16.9
Details

Potassium N-bromo-2,4-dichlorobenzenesulfonamidate sesquihydrate

B. Thimme Gowda,^a ^* Sabine Foro ^b and H. S. Spandana ^a

^aDepartment of Chemistry, Mangalore University, Mangalagangotri 574 199, Mangalore, India, and ^bInstitute of Materials Science, Darmstadt University of Technology, Petersenstrasse 23, D-64287 Darmstadt, Germany
Correspondence e-mail: gowdabt@yahoo.com

The asymmetric unit of the title salt, K⁺·C₆H₃BrCl₂NO₂S^-·1.5H₂O, contains one K⁺ cation, one N-bromo-2,4-dichlorobenzenesulfonamidate anion, one water molecule in general position and one water molecule located on a twofold rotation axis. The K⁺ cation is hepta-coordinated by three water O atoms and four sulfonyl O atoms from three symmetry-related N-bromo-2,4-dichlorobenzenesulfonamide anions. The S=N distance of 1.575 (3) Å is consistent with that of a double bond. In the crystal, the anions are linked by O-HBr and O-HN hydrogen bonds into layers parallel to the ac plane.

Related literature

For preparation of N-haloarylsulfonamides, see: Gowda & Mahadevappa (1983). For studies of the effect of substituents on the structures of N-haloarylsulfonamides, see: George et al. (2000); Gowda et al. (2007, 2011a,b); Olmstead & Power (1986).

Experimental

Crystal data

K⁺·C₆H₃BrCl₂NO₂S^-·1.5H₂O
M_r = 740.18
Monoclinic, C 2/c
a = 12.5263 (7) Å
b = 6.7638 (4) Å
c = 29.703 (2) Å
= 98.352 (5)°
V = 2489.9 (3) Å³
Z = 4
Mo K radiation
= 4.22 mm^-1
T = 293 K
0.32 × 0.32 × 0.28 mm

Data collection

Oxford Diffraction Xcalibur diffractometer with Sapphire CCD detector
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ) T_min = 0.345, T_max = 0.384
4960 measured reflections
2535 independent reflections
2204 reflections with I > 2(I)
R_int = 0.014

Refinement

R[F² > 2(F²)] = 0.037
wR(F²) = 0.093
S = 1.09
2535 reflections
150 parameters
3 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.76 e Å^-3
_min = -0.65 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O3-H31Br1ⁱ	0.80 (2)	2.78 (2)	3.550 (3)	160 (4)
O3-H32N1	0.81 (2)	2.15 (3)	2.917 (4)	158 (5)
O4-H41N1ⁱⁱ	0.82 (2)	2.16 (2)	2.957 (3)	165 (5)
Symmetry codes: (i) $[x+{\script{1\over 2}}, y-{\script{1\over 2}}, z]$ ; (ii) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

Data collection: CrysAlis CCD (Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NC2295 ).

Acknowledgements

BTG thanks the University Grants Commission, Government of India, New Delhi, for a one-time grant to Faculty/Professors under UGC-BSR.

References

George, E., Vivekanandan, S. & Sivakumar, K. (2000). Acta Cryst. C56, 1208-1209.
Gowda, B. T., Foro, S. & Shakuntala, K. (2011a). Acta Cryst. E67, m926.
Gowda, B. T., Foro, S. & Shakuntala, K. (2011b). Acta Cryst. E67, m962.
Gowda, B. T. & Mahadevappa, D. S. (1983). Talanta, 30, 359-362.
Gowda, B. T., Tokarcík, M., Kozísek, J. & Fuess, H. (2007). Acta Cryst. E63, m2115-m2116.
Olmstead, M. M. & Power, P. P. (1986). Inorg. Chem. 25, 4057-4058.
Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148-155.

metal-organic compounds